Metal iyonlarının 1, 10-ferontrolin ile kompleks oluşturarak kopiler elektroforez yöntemi ile ayrılması ve tayini
Başlık çevirisi mevcut değil.
- Tez No: 55500
- Danışmanlar: DOÇ.DR. BEDİA ERİM
- Tez Türü: Yüksek Lisans
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1996
- Dil: Türkçe
- Üniversite: İstanbul Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Belirtilmemiş.
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 53
Özet
ÖZET Bu çalışmada; Zn(II). Cu(II) ve Fe(II) iyonlarının 1, 10-Fenantrolin ligandı ile ön kolon kompleksi esmesi yöntemi uygulanarak, kapiler elektroforez ile ayrılmaları ve tespitleri gerçekleştirilmiştir. Ayırma yönteminin elektroforetik tampon parametreleri, deteksiyon limitleri ve tekrarlanabil iri ik verileri incelenmiştir. İyonlar pH=2.5'luk, kloroasetik asit tamponunda 6 dak. sürede ayrılmışlardır. Çalışma voltajı olarak 28 kV seçilmiştir. Deteksiyon 226 nm'de gerçekleştirilmiştir. Yöntemin vitamin tabletleri içindeki metal analizlerine uygulanması gösterilmiştir. vııı
Özet (Çeviri)
SUMMARY SEPARATION AND DETERMINATION OF METAL IONS COMPLEXED WITH 1,10 PHENANTHROLINE BY CAPILLARY ELECTROPHORESIS Capillary electrophoresis (CE) is recognized as a powerful new analytical separation tecnique. CE has es tablished itself as an important and widely utilized tecnique for routine analytical separations. Electrophoresis has been defined as the differential movement of charged species (ions) by attraction or re pulsion in an electric field. Electrophoresis as a sepa ration tecnique was introduced by Tiselius in 1937. Placing protein mixtures between buffer solutions in a tube and applying an electric field, he found that sample components migrated in a direction and at a rate deter mined by their charge and mobility. For his work in se paration science Tiselius was awarded a Nobel Prize. Separation effiency in free solution, as performed by Tiselius, was limited by thermal diffusion and convec tion. For this reason, electrophoresis traditionally has been performed in anti-convective media, such as poly- acrylamide or agorase gels. Gels in the slab or tube for mat have been used primarily for the size-dependent separation of biological macromolecules, such as nucleic acids and proteins. Although it is one of the most widely used separation tecniques, slab gel electrophoresis gene rally suffers from long analysis times, low efficiencies, and difficulties in detection and automation. An alternative to the slab-format is to perform the electrophoretic separation in norrow-bore tubes or ca pillaries. Since narrow capillaries are themselves anti- convective, gel media are not essential to perform that function. This allows the performance of free-solution (or open tube) electrophoresis, as well as the use of traditional gel media in the capillary [193. S Initial work in open tube elctrophoresis was de scribed by Hjerten in 1967 [23, 24].At that time, since only milimeter-bore capillaries were avaible, Hjerten -ix-rotated them along their longitudinal axis to minimize the effects of convection. Later Mikkers performed elec trophoresis in approximately 200-um internal diameter (id) capillaries made from glass and Teflon, respectively [25]. ~İn the early 1980s Jorgenson and Lukacs advanced the tecnique by using 75-wm id fused silica capillaries ' [261. Jorgenson also clarified the theory, described the relationships“ between operational parameters and separa tion quality, and demonstrated the potential of high per formance CE as an analytical tecnique. Since that time, numerous reviews and a few books have been written describing various aspects of CE [27]..In CE the separation compartment is a narrow ca pillary filled with an electrolyte solution. The electric field is applied with an external high-voltage. source between two electrodes in small vials in contact with the solution at both ends of a separation compartment. The sample iş introduced as a narrow band or zone at one end, and detection takes place near the other end of the ca pillary. The advantage over classical electro-phoresis, known already in the previous century, is mainly the high separation effiency of CE. Therefore the name high-per formance capillary electrophoresis (HPCE) is also used. The most common variant of CE is Capillary Zone Electrophoresis (CZE). Here, narrow zones of sample ions migrate with different velocities through a background electrolyte (BGE) in the capillary. Other variants of CE are for instance isotachophoresis (ITP) and capillary isoelectric focussing (CIEF). The difference with CZE is in the electrolytes used in the capillary and the vials; the instrumental set-up is the same. In other sub- techniques of CE, an extra separation principle is used apart from the electrophoretic effect. In capillary gel electrophoresis (CGE) the sieving effect of the gel is used for the separation of large ions. In micellar elec- trokinetic chromatography (MEKC), there is a distribution of neutral and charged sample components between the aqueous solution and micelles. Still, in all of these se- peration techniques the principles of electrophoresis are important [20].['”“”“ Separation by electrophoresis is based on differen ces in solute velocity in an electric field. The velocity of an ion can be given by; v - fi.£ where v - ion velocity /i£ - electrophoretic mobility E - applied electric field -x-The electric field is simply a function of the applied voltage and capillary length (in volts/cm.). The mobility of a spherical particle is given by : Q where q« ion charge Y\m solution viscosity r- ion radius From this equation it is evident that small, highly charged species have high mobilities whereas large, mini mally charged species have low mobilities. A fundamental constituent of CE operation is electro-osmotic, or electroendosmotic flow (EOF). When an aqueus solution of electrolytes, as used in electrophoresis, is in contact with the wall of the separation capillary, there is a charge difference between the wall and the solution. This can be caused by ionization of the wall meterial or by specific adsorption of ions from the solution to the wall. With fused silica capillaries the wall is usually negatively charged. Free silanol groups on the surface of the fused silica are deprotonated (at pH> 1.5), leaving negative Si-0 groups. Since the system as a whole must be electrically neutral, the solution in the separation compartment has a net positive charge. This excess of positive ions is located in the solution close to the wall, due to the electro static attraction by the negative wall. When a voltage is applied between the ends of the capillary, the electric field exerts a force on the excess of positive charge in the solution close to the wall. This force drives the solution in the capillary as a whole in the direction of the negative electrode. A constant flow of the solu tion results when the viscous forces in the thin layer of solution near the wall counterac the electrostatic force. This phenomenon is called electro-osmotic or electro-endosmotic flow (EOF). Electro-osmosis is an important feature of CE since the separation is performed in free solution. In classical electrophoresis with its highly viscous gels or agars, it generally does not play a role. The velocity of the electro-osmotic flow is propor tional to the field strength. An osmotic mobility can be defined: -xi-ti - Electroosmotic mobility It depends mainly on the wall material and the pH of the solution (who together determine the charge density on the wall) and on the viscosity of the solution. For a fus_ed silica capillary at pH 7 it is in the order of 50. 10”m2/V.s. Often the osmotic motility is larger than the ionic mobilities of the analytes in the solution. This implies that all solutes move towards the negative electrode, with a velocity: -for positive ions: v; - ( y.o + fjt, ).E -for negative ions: v - ( ^ - y.. ),E -for neutral particles: v - pt0. E Ionic components may reach the detector before or after the“osmotic flow peak”, depending on the direction of their migration relative to the osmotic flow. Their peak-times and mobilities are related by: L' L'. L (fi ± p. ). E (po i fi. ). v L'- effective capillary length (to the detector) L - total capillary length t ? migration time Increasing the length of the capillary has a double effect on the time of analysis: not only is the distance that that the zones have to cover increased but also the field strength is decreased. A number of detection methods have been used in CE. As in HPLC, UV-visible detection is bay-far the most corn- men. Fluoresence, laser induced fluoresence and electro chemical detection methods have been also extensively used. Other detection schemes such as mass and inducti vely coupled plasmas ( I CP) have been employed in the last years. -XI 1-Some excellent separations of various metal ions by CE have recently been demonstrated. Often, the separation is facilitated by addition of a weak complexing agent added to the capillary electrolyte to partially complex the sample cations. Another approach has been to complex metal ions completely by adding a strong complexing agent to the sample and then to separate the metal complexes by CE. Along with a possibility to detect metal ions by direct adsorbance measurements, this approach makes it possible to eliminate largely interferences from complex sample matrices, such as serum, pharmaceutical prepara tions, electroplating solutions, ores, etc [22]. In this study ZnCII), Cu(II) and Fe(II) ions were separated and detected following the pre-column formation of phenathroline complexes by CE with UV-detection. Elec- trophoretic buffer parameters, limit of detection, linear dynamic range and reproducubility of separation were exa mined. The mixture of metal complexes with phenanthroline were separated in about 6 minutes in a fused silica ca pillary column with a chloroasetic acid buffer of pH=2. 5 at an applied voltage of 28 kV, followed by direct UV- detection at 226 nm. The applicability of the method for the determination of metals in vitamin tablet is presen ted. -XI 11-
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